Ag is preferred over other metals as it is comparatively low-reactive, more stable and less expensive [93]. The optimized NW dispersion (Appendix B) with 0.3 % w/v of ZnO nanowires in DI water is drop-casted over the SiO2/Si substrate at a high temperature near 190◦C to avoid the agglomeration of NWs into random clusters due to high surface tension in DI water. The optimized ZnO SNWs solution helps to place the NWs at a reasonable distance on the substrate, which helps in targeting an SNW for printing metal contact pads to complete the device fabrication. AgNP contact pads are printed using MCP technology, which uses a molecular printing system (Make: BioForce Nanosciences) containing a surface patterning tool (SPT) consisting of a silicon micro-cantilever print-head [36, 55].
The micro-cantilever has a 5-10 µm wide micro-channels through which the ink to be printed flows or is temporarily stored. The micro-cantilever is typically 200 µm long and 30-60 µm wide. AgNP contact pads have been printed using SPT drag printing (SDP) and dip-ink printing with spot overwrite printing (DIPSOP) modes of micro-cantilever printing (MCP) technology [36].
The micro-cantilever tip can be used to perform SPT drag printing (SDP) and dip-ink printing with spot overwrite printing (DIPSOP) [36]. A schematic diagram showing the step-by-step process of DIPSOP and SDP technique is illusterd in Figure 3.3(a, b, and c) and Figure 3.3(d, e, and f), respectively. The micro-cantilever is kept under UV/O3 exposure for at least 30 minutes before using it for printing experiments to make the surface of micro-cantilever channels solvophilic to the AgNP ink to ensure that a large density of ink particles remain attached to it during the drag and dipping process [22]. After selecting a ZnO SNW,∼10 µL of AgNP ink is drop-casted as a local ink reservoir (LIR) ∼ 1000 µm away from one of the ends of the selected ZnO SNW. The micro-cantilever is positioned over the AgNP drop and slowly brought down using the coarse and fine z-axis control setting in NanoWare software installed with the printing system [55]. Initially, the focus of an optical camera attached to the printing software is to set much down the microcantilever to focus the drop and the SiO2/Si substrate. When the gap between the micro-cantilever and the drop reaches less than 100 µm, then both get focussed together. Further, the focus is re-adjusted to the tip of the micro- cantilever to avoid the spillover (proximity of micro-cantilever and drop may lead direct hit of whole surface pattering tool to the ink source). Fine z-axis control is used to move down slowly until the tip touches the AgNP drop peripheral region. When the micro-cantilever touches the upper surface of AgNP drop, ink particles diffuse inside its vacant micro-channels which reflects the solvophilic nature
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C.4 M-ZnO SNW based Schottky diode fabrication
of the cantilever. The micro-cantilever in touch with the ink-drop is dragged very slowly towards the targeted end of the ZnO SNW to a certain length (∼500-600µm). Then the micro-cantilever is slowly lifted to allow the ink captured inside its micro-channels to come out and get distributed over the dragged strip [36]. Dragged strip area acquires ink from LIR and thus results in a self-printing of contacts; the technique can be referred to as SDP assisted self-printing (SDP-SP).
Utilizing SDP-SP, a rectangular contact strip of AgNP is printed, overlapping one end of the ZnO SNW. The overlap is achieved by stopping the drag of the ink ∼ 2 to 5 µm before the ZnO SNW end and allowing the ink to automatically diffuse and self-print the remaining distance with the help of high ink-density gradient between the micro-cantilever dragged region and the gap-region between the AgNP ink and ZnO SNW of the substrate. Then the entire substrate is annealed from 50◦C to 200◦C with a rate of 8◦C/minute. If the overlap does not occur at the ZnO SNW interface region, two to three DIPSOP micro-spots of average diameter ∼5-10 µm are printed by ultra-fine position. The micro-spots ensures the targeted hit region such that 1-2µm of the peripheral region of the DIPSOP micro-spot touches the end of ZnO SNW without completely drowning the ZnO SNW with AgNP ink.
The DIPSOP spots are annealed properly to complete the fabrication of one-side of metal contact.
The steps, as mentioned earlier, are repeated to form the AgNP metal contacts to the other side of ZnO SNW.
To increase the scalability and ease of reproducibility of abovementioned printing technique, ZnO SNWs of longer lengths (>10µm) can be synthesized. It is relatively easy to print metal contact-pads with longer SNWs using SDP-SP and DIPSOP processes without any concerns of misalignment of micro-cantilever contact with the substrate or shorting between two metal pads. Therefore, following section discuss the fabrication of longer ZnO SNWs with help of acetic acid and SDS in optimized proportions with the ZnO dispersion DI water.
C.4 M-ZnO SNW based Schottky diode fabrication
Jang et al. have reported the synthesis of ZnO nanowires and nanorods with controlled morpholo- gies and aspect ratio in low-temperature hydrothermal conditions with the help of different forms of dodecyl sulfate, such as, sodium dodecyl sulfate (SDS) [95]. Choi et al. have also reported about the effect of SDS on the growth of ZnO particles by introducing doping of Na ions and improvement in the crystallinity and photoluminescence of fabricated ZnO nanostructures [94]. Similarly, Edinger et TH-2495_146102016
C. ZnO multiple and single NW based Schottky diode fabrication
Fig. C.2: Effect of acetic acid and SDS on morphology of ZnO NW (a) FESEM image showing formation of ZnO single-NWs with length> 10µm and width varying in range of ∼90 nm to 400 nm after addition of 1:3 acetic acid in ZnO NW dispersion in DI water and SDS (b) FESEM image showing improved separation between two ZnO NWs
al. have investigated the effect of Acetic acid on the growth rate, morphological and electro-optical properties of ZnO thin films and have found that Acetic acid favoured (001)-textured films and has an influence on the roughness and grain-size of the ZnO film [133]. Jiao et al. have also shown that Acetic acid has a great effect on the physical properties of ZnO thin films by enhancing their growth rate and modifying the surface morphology [134].
With the inputs from the above reports, 1 mg of SDS is added in 5 mL of DI water to lower down the surface tension of the solution. Further, 1.2 mL of this solution is taken out separately, and 2 mg of ZnO nanowire powder is dispersed in it. This ZnO NW dispersion is treated with Vortex generator for proper mixing. For simplicity, the ZnO NW dispersion in SDS-added DI water is abbreviated as low surface-tension nanowire dispersion (LST-NWD). 2 µL of this dispersion is added with the same amount of Acetic acid and drop-casted on the SiO2/Si substrate. It is observed that the addition of Acetic acid with LST-NWD in equal proportion can separate the individual ZnO NWs significantly and form longer (> 10 µm) ZnO NWs, having low-edge roughness, as shown in Figure C.2(a). It shows a small cluster of individual and longer ZnO NWs with lengths>10µm and width near 200-400 nm after addition of Acetic acid in 1:1 ratio with LST-NWD. To further decrease the width of above ZnO NWs, more Acetic acid is added in 3:1 ratio (6 µL of Acetic acid in 2 µL of LST-NWD). The addition of higher concentration of Acetic acid results in ZnO single-NWs with width near 100 nm and length greater than 10 µm with appreciable separation among individual nanowires as shown in Figure C.2(a, b). However, further addition of a higher concentration of Acetic acid results in the complete or partial dissolution of ZnO NWs in the acid. The ZnO SNWs synthesized using 3:1 ratio of
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C.4 M-ZnO SNW based Schottky diode fabrication
Acetic acid to LST-NWD got converted into ZnO micro-particles when heated at higher temperatures, near 250 ◦C. This shows that ZnO SNWs synthesized using a higher concentration of Acetic acid are not thermally stable and hence not suitable for sensing applications at higher temperatures. Therefore, 1:1 concentration of Acetic acid and ZnO NW dispersion in SDS-added DI water is considered as the optimized concentration to fabricate ZnO single-NW based devices for gas sensing applications. Since SDS and Acetic acid modify the structure of these ZnO NWs, these are referred to as Modified ZnO single nanowires (M-ZnO SNWs).
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C. ZnO multiple and single NW based Schottky diode fabrication
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D
Electron density computation
Contents
D.1 Computation for 1-D electron density using 1-D DOS for a ZnO SNW . . 134
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D. Electron density computation
D.1 Computation for 1-D electron density using 1-D DOS for a ZnO SNW
The electron density per unit length in a 1-D nanowire semiconductor can be written in energy space as [162]
nL=
∞
Z
Ec
f(E)D1d(E)dE (D.1)
where, D1d(E) is density of states in 1-D semiconductors like nanowire and is given as [162]
D1d(E) =
√2m∗
π~
r 1
E−Ec (D.2)
and m∗ is the effective mass of electrons in ZnO NW which is generally given asm∗= 0.39 me, where me is electron rest mass. Here, f(E) is the Fermi function given as
f(E) = 1
1 +eE−Ef/kBT (D.3)
where, Ec is the conduction band energy, ’kB’ is the Boltzmann constant,Ef is fermi level and T is the temperature in Kelvin. Putting (4,5) in (3), we get nLas follow
nL=
√ 2m∗ π~
∞
Z
Ec
√ dE
E−Ec(1 +eE−Ef/kBT) (D.4) Now, total electronic energy E can be expressed as follows assuming parabolic relation between electron energy and momentum
E =Ec+~2k2
2m∗ (D.5)
where,~2 is reduced plank’s constant given as~2=h/2π, ’k’ is the wave number. From above equation, we can express wave number ’k’ in terms of energy as
k=
p2m∗(E−Ec)
~
(D.6) Now, integrating fornL in terms of ’k’, we can write its expression as
nL=
√2m∗kBT π~
∞
Z
0
ε−1/2dε
1 +eε−nf (D.7)
where, εandnf are given as
ε=E−Ec/kBT (D.8)
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D.1 Computation for 1-D electron density using 1-D DOS for a ZnO SNW
nf =Ef −Ec/kBT (D.9)
Final expression for nL can be written as
nL=N1DF−1/2(nf) (D.10)
where,N1D is the effective density of states in 1-D nanowire andF−1/2(nf)is the Fermi-Dirac integral of order -1/2. These are expressed as follows
N1D = 1
~
r2m∗kBT
π (D.11)
F−1/2(nf) = 1
√π
∞
Z
0
ε−1/2dε
1 +eε−nf (D.12)
Since exact analytical solution forF−1/2 integral is not possible, we have used approximate solution of F−1/2(nf)integral as given below [162]
F−1/2(nf) =enf (D.13)
Hence, final expression ofnL can be written as
nL=N1Denf (D.14)
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D. Electron density computation
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